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Accessed from 10.6.1.

1 by JNJconsumer on Thu May 11 14:38:36 EDT 2017

2602 Adenosine / Official Monographs USP 40

ASSAY Acceptance criteria


• PROCEDURE Any individual impurity: NMT 1.0%
Mobile phase: Dissolve 2.0 g of monobasic potassium Total impurities: NMT 1.5%
phosphate in 800 mL of water. Add 5 mL of 1.0 M tet-
rabutylammonium dihydrogen phosphate, dilute with SPECIFIC TESTS
water to 980 mL, and mix. Add 20 mL of acetonitrile. • PH 〈791〉: 4.5–7.5
System suitability solution: 0.03 mg/mL each of USP • PARTICULATE MATTER IN INJECTIONS 〈788〉: It meets the re-
Adenosine RS and inosine dissolved in warm water (50° quirements for small-volume injections.
to 55°), and diluted with water • BACTERIAL ENDOTOXINS TEST 〈85〉: When the product is
Standard solution: 0.03 mg/mL of USP Adenosine RS used for rapid intravenous injection, it contains NMT
dissolved in warm water (50° to 55°), and diluted with 11.62 USP Endotoxin Units/mg of adenosine. When the
water to volume. Before addition of the warm water, if product is used for continuous peripheral intravenous in-
sodium chloride is present in the Injection, add 0.01 mL fusion, it contains NMT 5.95 USP Endotoxin Units/mg of
of a solution of sodium chloride (0.9 in 100) per mL of adenosine.
the anticipated final volume of the Standard solution. • OTHER REQUIREMENTS: It meets the requirements under
Sample solution: Nominally 0.03 mg/mL of adenosine, Injections and Implanted Drug Products 〈1〉.
from a suitable volume of Injection in water
Chromatographic system ADDITIONAL REQUIREMENTS
(See Chromatography 〈621〉, System Suitability.) • PACKAGING AND STORAGE: Preserve in tight, single-dose
Mode: LC containers, preferably of Type I glass, and store at con-
Detector: UV 254 nm trolled room temperature.
Column: 3.9-mm × 30-cm; packing L1 • USP REFERENCE STANDARDS 〈11〉
Flow rate: 2.5 mL/min USP Adenosine RS
Injection volume: 10 µL USP Endotoxin RS
Run time: 2.5 times the retention time of adenosine
System suitability
Samples: System suitability solution and Standard
solution
.

[NOTE—The relative retention times of inosine and Medical Air


adenosine are 0.43 and 1.0, respectively.]
Suitability requirements DEFINITION
Resolution: NLT 6.0 between adenosine and inosine, Medical Air is a natural or synthetic mixture of gases consist-
System suitability solution ing largely of nitrogen and oxygen. It contains NLT
Tailing factor: NMT 2.0 for the adenosine peak, Sys- 19.5% and NMT 23.5%, by volume, of oxygen (O2).
tem suitability solution
Relative standard deviation: NMT 1.5%, Standard IDENTIFICATION
solution • A. The paramagnetic signal exhibited by the Sample gas
Analysis in the Assay confirms the presence of oxygen.
USP Monographs

Samples: Standard solution and Sample solution • B. The Sample gas in the Assay meets the assay Accep-
Calculate the percentage of the labeled amount of tance criteria.
adenosine (C10H13N5O4) in the portion of Injection ASSAY
taken: • PROCEDURE
Result = (rU/rS) × (CS/CU) × 100 The certified standards called for in the following test are
listed in Reagents, Indicators, and Solutions.
rU = peak response from the Sample solution Zero gas: Nitrogen certified standard
rS = peak response from the Standard solution Span gas: 21% Oxygen certified standard. [NOTE—See
CS = concentration of USP Adenosine RS in the Reagents, Indicators, and Solutions.]
Standard solution (mg/mL) Sample gas: Medical Air
CU = nominal concentration of adenosine in the Mode: Paramagnetic oxygen measurement (see Medical
Sample solution (mg/mL) Gases Assay 〈415〉)
Acceptance criteria: 90.0%–110.0% Analysis: Determine the concentration of oxygen in
percentage by volume of Medical Air using a suitable
IMPURITIES paramagnetic analyzer.
• ORGANIC IMPURITIES Acceptance criteria: 19.5%–23.5% of oxygen by
Mobile phase, System suitability solution, Standard volume
solution, Chromatographic system, and System suit-
ability: Proceed as directed in the Assay. IMPURITIES
Sample solution: Nominally 0.3 mg/mL of adenosine See Impurities Testing in Medical Gases Assay 〈413〉. The de-
from a volume of Injection, in water tector tubes called for in the following tests are listed in
Analysis Reagents, Indicators, and Solutions.
Sample: Sample solution If the label indicates that Medical Air is a synthetic mixture
Calculate the percentage of each impurity in the vol- of oxygen and nitrogen, and where oxygen complies to
ume of Injection taken: Oxygen USP and Nitrogen complies to Nitrogen NF, then
the Impurities tests are not required.
Result = (rU/rT) × 100 • LIMIT OF CARBON DIOXIDE
Sample: Detector tube manufacturer’s recommended
rU = peak response for each impurity volume ±5% of Medical Air
rT = sum of the responses of all of the peaks Analysis: Pass the Sample through a carbon dioxide de-
tector tube at the rate specified for the tube by the
detector tube manufacturer.
Acceptance criteria: NMT 500 ppm
• LIMIT OF CARBON MONOXIDE
Sample: Detector tube manufacturer’s recommended
volume ±5% of Medical Air

Official from May 1, 2017


Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.
Accessed from 10.6.1.1 by JNJconsumer on Thu May 11 14:38:36 EDT 2017

USP 40 Official Monographs / Alanine 2603

Analysis: Pass the Sample through a carbon monoxide VB = Titrant volume consumed by the Blank (mL)
detector tube at the rate specified for the tube by the N = actual normality of the Titrant (mEq/mL)
detector tube manufacturer. F = equivalency factor, 89.09 mg/mEq
Acceptance criteria: NMT 10 ppm W = Sample weight (mg)
• LIMIT OF SULFUR DIOXIDE Acceptance criteria: 98.5%–101.5% on the dried basis
Sample: Detector tube manufacturer’s recommended
volume ±5% of Medical Air IMPURITIES
Analysis: Pass the Sample through a sulfur dioxide de- • RESIDUE ON IGNITION 〈281〉: NMT 0.15%
tector tube at the rate specified for the tube by the • CHLORIDE AND SULFATE, Chloride 〈221〉
detector tube manufacturer. Standard solution: 0.70 mL of 0.020 N hydrochloric
Acceptance criteria: NMT 5 ppm acid
• LIMIT OF NITRIC OXIDE AND NITROGEN DIOXIDE Sample: 1.0 g of Alanine
Sample: Detector tube manufacturer’s recommended Acceptance criteria: NMT 0.05%
volume ±5% of Medical Air • CHLORIDE AND SULFATE, Sulfate 〈221〉
Analysis: Pass the Sample through a nitric oxide–ni- Standard solution: 0.30 mL of 0.020 N sulfuric acid
trogen dioxide detector tube at the rate specified for Sample: 1.0 g of Alanine
the tube by the detector tube manufacturer. Acceptance criteria: NMT 0.03%
Acceptance criteria: NMT 2.5 ppm • IRON 〈241〉: NMT 30 ppm
• LIMIT OF WATER AND OIL
Analysis: Support one container in an inverted position Delete the following:
(with the valve at the bottom) for 5 min. Cautiously
open the valve slightly, maintaining the container in an •• HEAVY METALS, Method I 〈231〉: NMT 15 ppm• (Official 1-
inverted position. Vent the gas with a barely audible
.

Jan-2018)
flow against a stainless steel mirror for a few seconds. • RELATED COMPOUNDS
Acceptance criteria: No liquid is discernible on the Mobile phase: 0.008 N sulfuric acid solution
mirror. System suitability solution: A mixture of 0.05 mg/mL
ADDITIONAL REQUIREMENTS of USP Fumaric Acid RS, 0.05 mg/mL of USP Maleic
• PACKAGING AND STORAGE: Preserve in pressurized contain- Acid RS, and 3 mg/mL of USP Malic Acid RS in water
ers. Container connections shall be appropriate for air. Maleic acid standard solution: 0.05 mg/mL of USP
Adaptors shall not be used to connect containers to pa- Maleic Acid RS in water
tient use supply system piping or equipment. Malic acid standard solution: 3 mg/mL of USP Malic
• LABELING: Label states if Medical Air is a synthetic mix- Acid RS in water
ture of Oxygen USP and Nitrogen NF. Where it is piped Fumaric acid standard solution: 0.05 mg/mL of USP
directly from the collecting tank to the patient point of Fumaric Acid RS in water
use, label each outlet “Medical Air”. Sample solution: 100 mg/mL of Alanine in water
Chromatographic system
(See Chromatography 〈621〉, System Suitability.)

USP Monographs
Mode: LC
Detector: UV 214 nm
Column: 7.8-mm × 30-cm; 9-µm packing L17
.

Alanine Column temperature: 30°


Flow rate: 0.6 mL/min
Injection volume: 10 µL
System suitability
Sample: System suitability solution
[NOTE—See Table 1 for the relative retention times.]
Suitability requirements
C3H7NO2 89.09 Resolution: NLT 1.5 between maleic acid and malic
L-Alanine [56-41-7].
acid
DEFINITION Relative standard deviation: NMT 5.0% for each of
Alanine contains NLT 98.5% and NMT 101.5% of L-alanine fumaric acid, maleic acid, and malic acid
(C3H7NO2), calculated on the dried basis. Analysis
Samples: Standard solutions and Sample solution
IDENTIFICATION Calculate the percentage of each specified acid in the
• A. INFRARED ABSORPTION 〈197K〉 portion of Alanine taken:
ASSAY Result = (rU/rS) × (CS/CU) × 100
• PROCEDURE
Sample: 80 mg of Alanine rU = peak response of maleic acid, malic acid, or
Titrimetric system fumaric acid from the Sample solution
(See Titrimetry 〈541〉.) rS = peak response of maleic acid, malic acid, or
Mode: Direct titration fumaric acid from the corresponding
Titrant: 0.1 N perchloric acid VS Standard solution
Endpoint detection: Potentiometric CS = concentration of USP Maleic Acid RS, USP
Blank: 3 mL of formic acid in 50 mL of glacial acetic Malic Acid RS, or USP Fumaric Acid RS in the
acid corresponding Standard solution (mg/mL)
Analysis: Dissolve the Sample in a mixture of 3 mL of CU = concentration of Alanine in the Sample solution
formic acid and 50 mL of glacial acetic acid, and titrate (mg/mL)
with Titrant. Calculate the percentage of any unspecified impurity in
Calculate the percentage of L-alanine (C3H7NO2) in the the portion of Alanine taken:
portion of Alanine taken:
Result = (rU/rS) × (CS/CU) × 100
Result = [(VS − VB) × N × F × 100]/W
rU = peak response of any unspecified impurity
VS = Titrant volume consumed by the Sample (mL) from the Sample solution

Official from May 1, 2017


Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.